CN109609805A - A kind of preparation process of c-based nanomaterial enhancing low melting point composite material - Google Patents
A kind of preparation process of c-based nanomaterial enhancing low melting point composite material Download PDFInfo
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- CN109609805A CN109609805A CN201811549187.5A CN201811549187A CN109609805A CN 109609805 A CN109609805 A CN 109609805A CN 201811549187 A CN201811549187 A CN 201811549187A CN 109609805 A CN109609805 A CN 109609805A
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- melting point
- low melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C13/00—Alloys based on tin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
Abstract
The present invention provides a kind of preparation processes of c-based nanomaterial enhancing low melting point composite material, it is related to a kind of method of high tough composite soldering of redox graphene enhancing SnAgCu system using powder melting process preparation nickel particles modification, wherein reinforced phase Ni-rGO is prepared using ball milling-thermal decomposition method.Specific steps are as follows: rGO is placed in planetary ball mill ball milling, rGO and the Ni (CH of ball milling3COO)2.4H2O powder uniformly mixes in proportion, and mixture is placed in heating in tube furnace and obtains Ni-rGO;Ni-rGO is proportionally mixed with solder powder, then the mixing in tumbling ball mill;The solder powder mixed is packed into corundum crucible, then heats in Muffle furnace, the air-cooled composite soldering for obtaining Ni-rGO enhancing;The present invention prepares the high tough composite soldering of low melting point of the redox graphene enhancing of nickel nano particle modification using powder melting process, improves the intensity of material.
Description
Technical field
The invention belongs to field of composite material preparation, and in particular to a kind of c-based nanomaterial enhancing low melting point composite material
Preparation process.
Background technique
In the unleaded process of electronic package material, SnAgCu brazing filler metal is with its excellent mechanical strength, reliability quilt
It is considered one of the best substitute of lead-free brazing.However, being passed with the lightweight, miniaturization and multifunction of electronic product
The SnAgCu solder of system is no longer satisfied the demand of Current electronic product.Therefore, a kind of novel tough unleaded pricker of height is developed
Material is particularly important.
Preparing novel lead-free solder, especially nanoparticle by means of nanoparticle doped, microalloying enhances compound pricker
The preparation of material is to improve the effective way of lead-free brazing performance, it has also become current research hotspot.Enhance in nanoparticle unleaded
In composite soldering, c-based nanomaterial is considered as reason with its excellent mechanical property, physical property and high specific surface area
The reinforced phase thought.But its as it is easy to reunite existing for reinforced phase, engage weak outstanding problem still with parent metal and seriously restrict
The preparation of c-based nanomaterial enhancing composite leadless solder.Therefore a kind of low melting point of effective c-based nanomaterial enhancing is found
The preparation method of composite material is at key point to solve this problem.Currently, the patent of application number 201010167210.1 is adopted
The tinbase composite soldering of carbon nanotube enhancing is prepared for smelting process;Application number 201510624582.5 and 201410512972.9
Patent using powder metallurgic method be prepared for graphene enhancing tinbase composite soldering.
In the preparation process of composite soldering, traditional smelting process and powder metallurgic method are mainly used at present.For carbon-based
For nano material enhances SnAgCu system low-melting alloy, when using traditional smelting process, due to c-based nanomaterial and matrix
Biggish density contrast between metal will lead to floating reunion of reinforced phase etc., to can not make to enhance during smelting and pouring
The mutually Dispersed precipitate in parent metal, can not also play the effect of reinforcing.When using powder metallurgy process, powder metallurgical technique master
To be applied to the preparation of high temperature refractory material, and for the powder metallurgical technique of low melting material, at a lower temperature
Diffusion rate is very slow, is difficult effectively to be sintered, weak so as to cause combining between powder, it is difficult to form effective metallurgical bonding.
Therefore, the preparation method for further probing into new low melting point composite material is a urgent problem to be solved.
In high temperature superconducting materia preparation, due to being had a variety of defects using the sample of solid-state sintering preparation, Zhou Lianyuan
The powder melting process of the inventions such as scholar significantly improves the performance of superconductor.Relatively in such high-temperature material such as high-temperature superconductor
Using, but powder melting process grinding in terms of low melting material especially c-based nanomaterial enhancing low melting point composite material preparation
Study carefully and is also rarely reported.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation work of c-based nanomaterial enhancing low melting point composite material
Skill improves the intensity of material using the high tough composite soldering of low melting point of powder melting process preparation c-based nanomaterial enhancing.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
A kind of preparation process of c-based nanomaterial enhancing low melting point composite material, it is characterised in that: specific steps are as follows:
Step 1: ball-milling treatment: redox graphene being placed in ball milling in ball mill, the ratio of grinding media to material of ball milling is 50:1, revolving speed
For 500r/min, Ball-milling Time 3h;
Step 2: by redox graphene and Ni (CH after ball milling 3h3COO)2·4H2O powder uniformly mixes by a certain percentage
It closes, the mixture being mixed to get is being connected with N2It is heated in the tube furnace of atmosphere, heating time 2h, heating temperature is 500 DEG C, N2
Gas flow is 800-1000mL/min, and furnace cooling after heating obtains the reduction-oxidation graphite of nickel nano particle modification
Alkene;
Step 3: the redox graphene of the nickel nano particle modification of step 2 preparation is added in low melting point solder powder,
30min is ultrasonically treated in alcoholic solution, the redox graphene of nickel nano particle modification is mixed with low melting point solder powder;
Step 4: the mixture of low melting point solder powder and the redox graphene of nickel nano particle modification is poured into ball grinder
In, the revolving speed of ball grinder is 100r/min, and Ball-milling Time 10h obtains mixed-powder;
Step 5: the mixed-powder that step 4 is obtained is packed into corundum crucible, it is then placed into and is connected with N2In the Muffle furnace of atmosphere
250 DEG C of heating 1h are cooled down the crucible for filling liquid solder in air to get nickel nano particle modification is arrived after heating
The low melting point composite soldering of redox graphene enhancing.
Further, the low melting point solder powder is low melting point SnAgCu brazing filler metal powder.
Further, the low melting point SnAgCu brazing filler metal powder is Sn2.5Ag0.7Cu0.1RE solder powder.
Further, the ball mill of step 1 is planetary ball mill.
Further, the redox graphene in step 2 and Ni (CH3COO)2·4H2In the mixture of O powder, Ni
Molar percentage be 10%.
Further, in step 3, the partial size of solder powder is 25-40 μm.
Further, in step 3, the additive amount in solder powder of the redox graphene of nickel nano particle modification
Mass fraction be 0.01wt.%~0.10wt.%.
Further, the ball grinder of step 4 is roller milling tank.
Further, the corundum crucible in step 5 is cylindrical crucible.
Further, the diameter of the corundum crucible is φ 20mm.
In the present invention, c-based nanomaterial and metal nanoparticle are respectively with redox graphene (rGO) and Ni nanometers
For particle, the eutectic of redox graphene (Ni-rGO) enhancing of nickel nano particle modification is prepared using powder melting process
The high tough composite soldering of point SnAgCu system, specifically using Ni-rGO as reinforced phase, by ball milling-thermal decomposition method in carbon-based nano
Material surface adhesion metal nanoparticle reduces the density contrast between reinforced phase and basis material, and improves and parent metal
Bond strength.Reinforced phase is mixed with parent metal solder powder, using powder melting process preparation c-based nanomaterial enhancing
Low melting point composite material can not only make reinforced phase Dispersed precipitate, but also guarantee effective combination between reinforced phase and matrix, to mention
Its high comprehensive performance.Reinforced phase of the Ni-rGO as solder improves the intensity of material using its excellent mechanical property.
The invention has the benefit that
1, the preparation process of a kind of c-based nanomaterial of the invention enhancing low melting point composite material, to redox graphene
(rGO) it carries out in metallizing process, this patent proposes a kind of completely new graphene surface modification method: ball milling-heat point
Solution heats the mixture of presoma and ball milling rGO, makes being attached to for Ni uniform particle specifically using nickel acetate as presoma
On rGO;Compared to traditional chemical plating method, ball milling-thermal decomposition method graphene surface method for metallising completely new as one kind,
This method is easy to operate, high-efficient, and the not pollution of heavy metal ion;The agglomeration traits of reinforced phase are efficiently solved, in turn
The tensile strength of composite soldering is improved, meanwhile, the addition of the redox graphene (Ni-rGO) of nickel nano particle modification can
The effective wetability for improving composite soldering;
2, the preparation process of a kind of c-based nanomaterial of the invention enhancing low melting point composite material, in the preparation of composite soldering
Cheng Zhong, in traditional smelting process and powder metallurgic method, there are disadvantages, and the invention proposes one kind to be used for low melting point composite material
Preparation method, i.e. powder melting process;Compared to powder metallurgic method, powder melting process reaches liquid phase state, atom due to solder
Diffusion rapidly, and can form effective metallurgical bonding;Compared to traditional smelting process, since heating temperature is low, liquid metal is viscous
Consistency is big, and the method does not have the casting process of liquid metal, therefore can keep the Dispersed precipitate of reinforced phase to greatest extent.
And when parent metal is under liquid condition, the Ni particle in Ni-rGO can quickly form Ni with Sn3Sn4Phase, and Ni and stone
Black alkene combination energy with higher, thus using powder melting process prepare composite soldering when, Ni-rGO can effectively play load
The effect of lotus transmitting.Based on the above reasons, the low melting point SnAgCu system that can obtain Ni-rGO enhancing using powder melting process is high
Tough composite soldering.
Detailed description of the invention
The TEM figure that Fig. 1 is Ni-rGO in embodiment 1;
Fig. 2 is that the SEM of Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy schemes;
Fig. 3 is the SEM figure that 0.05wt.%Ni-rGO enhances composite soldering in embodiment 3;
Fig. 4 be Sn3.0Ag0.5Cu solder, Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy and embodiment 1, embodiment 2,
The spreading area contrast schematic diagram of composite soldering in embodiment 3, embodiment 4;
Fig. 5 be Sn3.0Ag0.5Cu solder, Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy and embodiment 1, embodiment 2,
The tensile strength and elongation contrast schematic diagram of composite soldering in embodiment 3, embodiment 4.
Specific embodiment
In order to which those skilled in the art better understood when technical solution provided by the present invention, below with reference to specific
Embodiment income illustrates.
Embodiment 1
Step 1: ball-milling treatment: the rGO of 500mg being taken to be placed in ball-milling treatment in planetary ball mill, mill ball quality 25g, setting
Revolving speed is 500r/min, Ball-milling Time 3h.
Step 2: taking the rGO400mg of ball milling 3h, Ni (CH is taken3COO)2·4H2O powder 830mg, in planetary ball mill
In uniformly mix, mixture is being connected with N2500 DEG C of heating 2h in atmosphere tube type furnace, gas flow 900mL/min are cold with furnace
But to get arrive Ni-rGO.
Step 3: weighing the Sn2.5Ag0.7Cu0.1RE solder powder of 99.99g, partial size is 25-40 μm;Take certain content
Ni-rGO 30min is ultrasonically treated in alcoholic solution, then mixed with Sn2.5Ag0.7Cu0.1RE solder powder, wherein
The additive amount mass fraction of Ni-rGO is 0.01wt.%.
Step 4: the mixture of Sn2.5Ag0.7Cu0.1RE solder powder and Ni-rGO in step 3 are poured into drum-type
In ball grinder, setting revolving speed is 100r/min, Ball-milling Time 10h.
Step 5: the solder powder mixed is packed into the cylindrical corundum crucible that diameter is φ 20mm, it is then placed into
It is connected with N2250 DEG C of heating 1h in the muffle furnace of atmosphere, by the crucible for filling liquid solder it is air-cooled to get to Ni-rGO enhancing
Sn2.5Ag0.7Cu0.1RE composite soldering.Separately the Sn3.0Ag0.5Cu solder of 100g is prepared as reference.
Embodiment 2
Step 1: ball-milling treatment: the rGO of 500mg being taken to be placed in ball-milling treatment in planetary ball mill, mill ball quality 25g, setting
Revolving speed is 500r/min, Ball-milling Time 3h.
Step 2: taking the rGO400mg of ball milling 3h, Ni (CH is taken3COO)2·4H2O powder 830mg, in planetary ball mill
In uniformly mix, mixture is being connected with N2500 DEG C of heating 2h in atmosphere tube type furnace, gas flow 900mL/min are cold with furnace
But to get arrive Ni-rGO.
Step 3: weighing the Sn2.5Ag0.7Cu0.1RE solder powder of 99.99g, partial size is 25-40 μm;Take certain content
Ni-rGO 30min is ultrasonically treated in alcoholic solution, then mixed with Sn2.5Ag0.7Cu0.1RE solder powder, wherein
The additive amount mass fraction of Ni-rGO is 0.03wt.%.
Step 4: the mixture of Sn2.5Ag0.7Cu0.1RE solder powder and Ni-rGO in step 3 are poured into drum-type
In ball grinder, setting revolving speed is 100r/min, Ball-milling Time 10h.
Step 5: the solder powder mixed is packed into the cylindrical corundum crucible that diameter is φ 20mm, it is then placed into
It is connected with N2250 DEG C of heating 1h in the muffle furnace of atmosphere, by the crucible for filling liquid solder it is air-cooled to get to Ni-rGO enhancing
Sn2.5Ag0.7Cu0.1RE composite soldering.
Embodiment 3
Step 1: ball-milling treatment: the rGO of 500mg being taken to be placed in ball-milling treatment in planetary ball mill, mill ball quality 25g, setting
Revolving speed is 500r/min, Ball-milling Time 3h.
Step 2: taking the rGO400mg of ball milling 3h, Ni (CH is taken3COO)2·4H2O powder 830mg, in planetary ball mill
In uniformly mix, mixture is being connected with N2500 DEG C of heating 2h in atmosphere tube type furnace, gas flow 900mL/min are cold with furnace
But to get arrive Ni-rGO.
Step 3: weighing the Sn2.5Ag0.7Cu0.1RE solder powder of 99.99g, partial size is 25-40 μm;Take certain content
Ni-rGO 30min is ultrasonically treated in alcoholic solution, then mixed with Sn2.5Ag0.7Cu0.1RE solder powder, wherein
The additive amount mass fraction of Ni-rGO is 0.05wt.%.
Step 4: the mixture of Sn2.5Ag0.7Cu0.1RE solder powder and Ni-rGO in step 3 are poured into drum-type
In ball grinder, setting revolving speed is 100r/min, Ball-milling Time 10h.
Step 5: the solder powder mixed is packed into the cylindrical corundum crucible that diameter is φ 20mm, it is then placed into
It is connected with N2250 DEG C of heating 1h in the muffle furnace of atmosphere, by the crucible for filling liquid solder it is air-cooled to get to Ni-rGO enhancing
Sn2.5Ag0.7Cu0.1RE composite soldering.
Embodiment 4
Step 1: ball-milling treatment: the rGO of 500mg being taken to be placed in ball-milling treatment in planetary ball mill, mill ball quality 25g, setting
Revolving speed is 500r/min, Ball-milling Time 3h.
Step 2: taking the rGO400mg of ball milling 3h, Ni (CH is taken3COO)2·4H2O powder 830mg, in planetary ball mill
In uniformly mix, mixture is being connected with N2500 DEG C of heating 2h in atmosphere tube type furnace, gas flow 900mL/min are cold with furnace
But to get arrive Ni-rGO.
Step 3: weighing the Sn2.5Ag0.7Cu0.1RE solder powder of 99.99g, partial size is 25-40 μm;Take certain content
Ni-rGO 30min is ultrasonically treated in alcoholic solution, then mixed with Sn2.5Ag0.7Cu0.1RE solder powder, wherein
The additive amount mass fraction of Ni-rGO is 0.10wt.%.
Step 4: the mixture of Sn2.5Ag0.7Cu0.1RE solder powder and Ni-rGO in step 3 are poured into drum-type
In ball grinder, setting revolving speed is 100r/min, Ball-milling Time 10h.
Step 5: the solder powder mixed is packed into the cylindrical corundum crucible that diameter is φ 20mm, it is then placed into
It is connected with N2250 DEG C of heating 1h in the muffle furnace of atmosphere, by the crucible for filling liquid solder it is air-cooled to get to Ni-rGO enhancing
Sn2.5Ag0.7Cu0.1RE composite soldering.
In conjunction with the concrete analysis of attached drawing are as follows: Fig. 1 is the TEM picture of Ni-rGO in embodiment 1, and as can be seen from the figure Ni receives
Rice corpuscles is uniformly carried on rGO.
Fig. 2 and Fig. 3 is respectively 0.05 wt.%Ni-rGO increasing in Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy and embodiment 3
The SEM picture of strong Sn2.5Ag0.7Cu0.1RE composite soldering, it can be seen from the figure that with the addition of Ni-rGO, eutectic structure
Increase, β-Sn particle size is in the trend that is gradually reduced, and by ellipticity, gradually transition is round shape to β-Sn shape.
Fig. 4 is Sn3.0Ag0.5Cu solder, Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy and embodiment 1, embodiment 2, implements
The spreading area contrast schematic diagram of composite soldering in example 3, embodiment 4.From the figure 3, it may be seen that with the addition of Ni-rGO, spreading area
In different degrees of increase trend, when Ni-rGO additive amount is 0.05wt.%, sprawl up to maximum value 53.8mm2, than not adding
When improve 36.5%;And it is higher than the spreading area of Sn3.0Ag0.5Cu brazing alloy.
Fig. 5 is Sn3.0Ag0.5Cu solder, Sn2.5Ag0.7Cu0.1RE brazing filler metal alloy and embodiment 1, embodiment 2, implements
The tensile strength and elongation contrast schematic diagram of composite soldering in example 3, embodiment 4.As shown in Figure 4, with the increase of additive amount,
The tensile strength that Ni-rGO enhances Sn2.5Ag0.7Cu0.1RE composite soldering shows first increases and then decreases trend, corresponding elongation
In gradually decreasing trend.When Ni-rGO additive amount is 0.05wt.%, tensile strength reaches maximum value 58.1MPa, compares
Sn2.5Ag0.7Cu0.1RE improves 15.0%, compound at this time also above the tensile strength of commercial Sn3.0Ag0.5Cu solder
Solder elongation is 33.8%.Obtain high tough Ni-rGO enhancing Sn2.5Ag0.7Cu0.1RE composite soldering.
In addition, in conjunction with the embodiments 1,2,3,4 and Fig. 2~5 it can also be seen that when Ni-rGO additive amount be 0.05wt.% when,
The structure refinement of composite soldering, spreading area and tensile strength reach most preferably, and elongation is in the best of 30% or more, Ni-rGO
Additive amount is 0.05wt.%.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
The present invention will not be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty
The consistent widest scope of point.
Claims (10)
1. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material, it is characterised in that: specific steps are as follows:
Step 1: ball-milling treatment: redox graphene being placed in ball milling in ball mill, the ratio of grinding media to material of ball milling is 50:1, revolving speed
For 500 r/min, Ball-milling Time 3h;
Step 2: by redox graphene and Ni (CH after ball milling 3h3COO)2×4H2O powder uniformly mixes by a certain percentage
It closes, the mixture being mixed to get is being connected with N2It is heated in the tube furnace of atmosphere, heating time 2h, heating temperature is 500 DEG C, N2
Gas flow is 800-1000mL/min, and furnace cooling after heating obtains the reduction-oxidation graphite of nickel nano particle modification
Alkene;
Step 3: the redox graphene of the nickel nano particle modification of step 2 preparation is added in low melting point solder powder,
30min is ultrasonically treated in alcoholic solution, the redox graphene of nickel nano particle modification is mixed with low melting point solder powder;
Step 4: the mixture of low melting point solder powder and the redox graphene of nickel nano particle modification is poured into ball grinder
In, the revolving speed of ball grinder is 100r/min, and Ball-milling Time 10h obtains mixed-powder;
Step 5: the mixed-powder that step 4 is obtained is packed into corundum crucible, it is then placed into and is connected with N2In the Muffle furnace of atmosphere
The crucible for filling liquid solder is cooled down in air after heating and is modified to get to nickel nano particle by 250 DEG C of 1 h of heating
Redox graphene enhancing low melting point composite soldering.
2. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
Be: the low melting point solder powder is low melting point SnAgCu brazing filler metal powder.
3. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 2, feature
Be: the low melting point SnAgCu brazing filler metal powder is Sn2.5Ag0.7Cu0.1RE solder powder.
4. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
Be: the ball mill of step 1 is planetary ball mill.
5. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
It is: redox graphene and Ni (CH in step 23COO)2×4H2In the mixture of O powder, the molar percentage of Ni
It is 10%.
6. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
Be: in step 3, the partial size of solder powder is 25-40 μm.
7. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1 or 6, special
Sign is: in step 3, the mass fraction of additive amount in solder powder of the redox graphene of nickel nano particle modification
For 0.01wt.% ~ 0.10wt.%.
8. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
Be: the ball grinder of step 4 is roller milling tank.
9. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 1, feature
Be: the corundum crucible in step 5 is cylindrical crucible.
10. a kind of preparation process of c-based nanomaterial enhancing low melting point composite material according to claim 9, feature
Be: the diameter of the corundum crucible is 20 mm of φ.
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Application publication date: 20190412 Assignee: Luoyang Lei Jia Electronic Technology Co.,Ltd. Assignor: HENAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2021980015165 Denomination of invention: Preparation process of carbon based nano material reinforced low melting point composite Granted publication date: 20210702 License type: Common License Record date: 20211222 |